CN102951622B - Preparation method of diammonium phosphate by acid slurry co-production - Google Patents
Preparation method of diammonium phosphate by acid slurry co-production Download PDFInfo
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- CN102951622B CN102951622B CN201210402974.3A CN201210402974A CN102951622B CN 102951622 B CN102951622 B CN 102951622B CN 201210402974 A CN201210402974 A CN 201210402974A CN 102951622 B CN102951622 B CN 102951622B
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- phosphoric acid
- diammonium phosphate
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Abstract
The invention discloses a preparation method of diammonium phosphate by acid slurry co-production. The method comprises the following steps of: introducing ammonia into diluted phosphoric acid with concentration between 22.0 and 24.0 percent; feeding the diluted phosphoric acid into a peripheral circulation evaporator, a double-effect heat exchanger and a single-effect heat exchanger sequentially to prepare acid slurry; introducing ammonia into strong phosphoric acid with concentration between 35.0 and 40.0 percent to prepare the strong phosphoric acid with neutralization degree between 0.4 and 0.7; mixing the acid slurry and the strong phosphoric acid in a volume ratio of 1: (3-5), and feeding into an acid pump to prepare a phosphoric acid slurry mixed liquid; feeding the mixed liquid into a neutralization tank, introducing ammonia into the neutralization tank to perform an ammonization-granulation reaction to prepare neutralized slurry; and feeding the neutralized slurry into a granulator to perform an ammonized granulation process to prepare diammonium phosphate particles; and drying and dehydrating the diammonium phosphate particles, and grading and screening to obtain diammonium phosphate particles. According to the preparation method, the problems of hard control on N and P contents and low energy output in the diammonium phosphate production method by the traditional method can be solved.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of preparation method of acid slime co-producing diammonium phosphate.
Background technology
Existing Traditional Method production diammonium phosphate, strong phosphoric acid concentration basic controlling is at 35.0%-45.0%, when phosphoric acid concentration is too low, the phosphor ammonium slurry water content that neutralization reaction generates is bigger than normal, the diammonium phosphate granule strength that granulation generates is poor, and the finished product moisture is high, and the content of N, P is low; When phosphoric acid concentration is too high, the phosphor ammonium slurry water content that neutralization reaction generates is less than normal, and the product of the diammonium phosphate that granulation is produced is many from granulating, and visual appearance is poor, the content of the final N of product, P is high, so the N to diammonium phosphate, the control of P content are directly determining the quality of quality product.
In traditional method, for the stable content of controlling product N, P, a kind of is to adopt the strong phosphoric acid of high density and the method that phosphorus ammonium washing tail gas water is blent, strong phosphoric acid concentration is controlled to a certain desired value, in use, wet-process phosphoric acid concentration system must first be produced the strong phosphoric acid of high density to this method, and then with washing water blend reduce acid dense, make concentrating unit resource serious waste, production capacity is low; Another kind is solid content and the SO by adjusting strong phosphoric acid
3the method of content, this method in use content of N, P is not easy to control, and makes the outward appearance of product because being subject to the impact of solid content can not keep stable simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of acid slime co-producing diammonium phosphate, be not easy to control the problem that production capacity is low to solve the content of Traditional Method N, P in production diammonium phosphate process.
The technical solution adopted in the present invention is: a kind of preparation method of acid slime co-producing diammonium phosphate, implements according to following steps:
Step 1, passes into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 22.0%-24.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, makes the dilute phosphoric acid that degree of neutralization is 0.95-1.05; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-50--70kPa to make the acid slime that proportion is 1.45-1.55 again;
Step 2, passes into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 35.0%-40.0%, makes the strong phosphoric acid that degree of neutralization is 0.4-0.7;
Step 3, after the ratio that is by volume 1:3-5 dissolves, sends into sour pump by the strong phosphoric acid making in the acid slime making in step 1 and step 2, makes phosphoric acid material pulp mixing solutions;
Step 4, sends the phosphoric acid material pulp mixing solutions making in step 3 into neutralizing well, simultaneously in neutralizing well, sends into ammonia, carries out ammoniation-granulation reaction, in making and slip;
Step 5, carries out ammoniation and granulation technique by sending into tablets press with slip in making in step 4, makes diammonium phosphate particle;
Step 6, carries out drying and dehydrating by the diammonium phosphate particle making in step 5, then its gradation sizing is obtained to diammonium phosphate particle.
Feature of the present invention is also,
Wherein in step 4, the volume ratio of ammonia and phosphoric acid material pulp mixing solutions is 210-230:1.
Wherein in step 6, the particle diameter of the diammonium phosphate after screening is 2-4mm.
The invention has the beneficial effects as follows: by the preparation method of acid slime co-producing diammonium phosphate, the content that has solved Traditional Method N, P in production diammonium phosphate process is not easy to control, the problem that production capacity is low.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
The invention provides a kind of preparation method of acid slime co-producing diammonium phosphate, specifically implement according to following steps:
Step 1, passes into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 22.0%-24.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, makes the dilute phosphoric acid that degree of neutralization is 0.95-1.05; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-50--70kPa to make the acid slime that proportion is 1.45-1.55 again;
Step 2, passes into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 35.0%-40.0%, makes the strong phosphoric acid that degree of neutralization is 0.4-0.7;
Step 3, after the ratio that is by volume 1:3-5 dissolves, sends into sour pump by the strong phosphoric acid making in the acid slime making in step 1 and step 2, makes phosphoric acid material pulp mixing solutions;
Step 4, sends the phosphoric acid material pulp mixing solutions making in step 3 into neutralizing well, and the volume ratio that is 210-230:1 by ammonia and this phosphoric acid material pulp mixing solutions is sent into ammonia in neutralizing well, carries out ammoniation-granulation reaction, in making and slip;
Step 5, carries out ammoniation and granulation technique by sending into tablets press with slip in making in step 4, makes diammonium phosphate particle;
Step 6, carries out drying and dehydrating by the diammonium phosphate particle making in step 5, then its gradation sizing is obtained to 2-4mm diammonium phosphate particle.
Embodiment mono-
Pass into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 24.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, make degree of neutralization and be 1 dilute phosphoric acid; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-70kPa again, makes proportion and be 1.50 acid slime; Pass into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 40.0%, make degree of neutralization and be 0.55 strong phosphoric acid; The acid slime making and strong phosphoric acid, by volume for after the ratio of 1:3 dissolves, are sent into sour pump, make phosphoric acid material pulp mixing solutions; This phosphoric acid material pulp mixing solutions is sent into neutralizing well, and the ratio that is 230:1 in the volume ratio of ammonia and this phosphoric acid material pulp mixing solutions is sent into ammonia in neutralizing well, carries out ammoniation-granulation reaction, in making and slip; Carry out ammoniation and granulation technique by sending into tablets press with slip in this, make diammonium phosphate particle; This diammonium phosphate particle is carried out to drying and dehydrating, then its gradation sizing is obtained to 2-4mm diammonium phosphate particle.
Embodiment bis-
Pass into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 23.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, make degree of neutralization and be 1.05 dilute phosphoric acid; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-60kPa again, makes proportion and be 1.55 acid slime; Pass into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 37.5%, make degree of neutralization and be 0.7 strong phosphoric acid; The acid slime making and strong phosphoric acid, by volume for after the ratio of 1:5 dissolves, are sent into sour pump, make phosphoric acid material pulp mixing solutions; This phosphoric acid material pulp mixing solutions is sent into neutralizing well, and the ratio that is 220:1 in the volume ratio of ammonia and this phosphoric acid material pulp mixing solutions is sent into ammonia in neutralizing well, carries out ammoniation-granulation reaction, in making and slip; Carry out ammoniation and granulation technique by sending into tablets press with slip in this, make diammonium phosphate particle; This diammonium phosphate particle is carried out to drying and dehydrating, then its gradation sizing is obtained to 2-4mm diammonium phosphate particle.
Embodiment tri-
Pass into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 22.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, make degree of neutralization and be 0.95 dilute phosphoric acid; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-50kPa again, makes proportion and be 1.45 acid slime; Pass into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 35.0%, make degree of neutralization and be 0.4 strong phosphoric acid; The acid slime making and strong phosphoric acid, by volume for after the ratio of 1:4 dissolves, are sent into sour pump, make phosphoric acid material pulp mixing solutions; This phosphoric acid material pulp mixing solutions is sent into neutralizing well, and the ratio that is 210:1 in the volume ratio of ammonia and this phosphoric acid material pulp mixing solutions is sent into ammonia in neutralizing well, carries out ammoniation-granulation reaction, in making and slip; Carry out ammoniation and granulation technique by sending into tablets press with slip in this, make diammonium phosphate particle; This diammonium phosphate particle is carried out to drying and dehydrating, then its gradation sizing is obtained to 2-4mm diammonium phosphate particle.
In traditional method, for the stable content of controlling product N, P, a kind of is to adopt the strong phosphoric acid of high density and the method that phosphorus ammonium washing tail gas water is blent, strong phosphoric acid concentration is controlled to a certain desired value, this method in use wet-process phosphoric acid concentration system must first be produced the strong phosphoric acid of high density, and then with washing water blend reduce acid dense, make concentrating unit resource serious waste, production capacity is low; Another kind is solid content and the SO by adjusting strong phosphoric acid
3the method of content, this method in use content of N, P is not easy to control, and makes the outward appearance of product because being subject to the impact of solid content can not keep stable simultaneously.
And in the preparation method's of acid slime co-producing diammonium phosphate of the present invention production process, can directly reduce the content of product N, P by increasing the consumption of acid slime, or improve the content of product N, P by reducing the consumption of acid slime, in the process of this regulation and control product N, P content, the indices of the strong phosphoric acid using remains constant, strengthen the effect that regulates and controls diammonium phosphate N, P content, made the outward appearance of product more mellow and fuller simultaneously, improved the visual appearance of product.
In produced in conventional processes diammonium phosphate process, the production capacity of the strong phosphoric acid taking quality of production concentration per hour as 40% is as 10m
3for example, 12.5 tons of the diammonium phosphate of producing per hour.And in the preparation method's of acid slime co-producing diammonium phosphate of the present invention production process, only needing to provide mass concentration is 35% strong phosphoric acid, production capacity per hour is 11.4m
3, dissolving ratio according to strong phosphoric acid and acid slime is that 3:1 calculates, so, and 11.4m
3strong phosphoric acid can dissolve use 3.8m
3acid slime, amounting to per hourly can provide 15.2m
3phosphoric acid material pulp mixing solutions send into neutralizing well, 18 tons of the diammonium phosphate of producing per hour, output has improved 44% than Traditional Method production diammonium phosphate.
Claims (1)
1. a preparation method for acid slime co-producing diammonium phosphate, is characterized in that, implements according to following steps:
Step 1, passes into ammonia to the dilute phosphoric acid that in dilute phosphoric acid circulation acid tank, mass concentration is 22.0%-24.0%, then this dilute phosphoric acid is sent to outside circulation vaporizer, makes the dilute phosphoric acid that degree of neutralization is 0.95-1.05; This dilute phosphoric acid is sent into successively to two effect interchanger and an effect interchanger, the vacuum tightness of simultaneously controlling two effect interchanger is-50--70kPa to make the acid slime that proportion is 1.45-1.55 again;
Step 2, passes into ammonia to the strong phosphoric acid that in strong phosphoric acid circulation acid tank, mass concentration is 35.0%-40.0%, makes the strong phosphoric acid that degree of neutralization is 0.4-0.7;
Step 3, after the ratio that is by volume 1:3-5 dissolves, sends into sour pump by the strong phosphoric acid making in the acid slime making in step 1 and step 2, makes phosphoric acid material pulp mixing solutions;
Step 4, sends the phosphoric acid material pulp mixing solutions making in step 3 into neutralizing well, simultaneously in neutralizing well, sends into ammonia, carries out ammoniation-granulation reaction, in making and slip; The volume ratio of described ammonia and phosphoric acid material pulp mixing solutions is 210-230:1;
Step 5, carries out ammoniation and granulation technique by sending into tablets press with slip in making in step 4, makes diammonium phosphate particle;
Step 6, carries out drying and dehydrating by the diammonium phosphate particle making in step 5, then its gradation sizing is obtained to diammonium phosphate, and the particle diameter of the diammonium phosphate after described screening is 2-4mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210402974.3A CN102951622B (en) | 2012-10-18 | 2012-10-18 | Preparation method of diammonium phosphate by acid slurry co-production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210402974.3A CN102951622B (en) | 2012-10-18 | 2012-10-18 | Preparation method of diammonium phosphate by acid slurry co-production |
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| CN102951622A CN102951622A (en) | 2013-03-06 |
| CN102951622B true CN102951622B (en) | 2014-10-01 |
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| CN105236374B (en) * | 2015-09-16 | 2018-03-13 | 贵州开磷集团股份有限公司 | A kind of preparation method of granular diammonium phosphate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226544A (en) * | 1999-01-15 | 1999-08-25 | 铜陵化学工业集团公司磷铵厂 | Method and apparatus for producing diammonium phosphate with external circulation ammoniation reactor |
| CN1872669A (en) * | 2006-06-16 | 2006-12-06 | 四川川大中德环保技术有限公司 | Method for producing diammonium phosphate by concentrating acid slime, and secondary ammoniation reactor |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226544A (en) * | 1999-01-15 | 1999-08-25 | 铜陵化学工业集团公司磷铵厂 | Method and apparatus for producing diammonium phosphate with external circulation ammoniation reactor |
| CN1872669A (en) * | 2006-06-16 | 2006-12-06 | 四川川大中德环保技术有限公司 | Method for producing diammonium phosphate by concentrating acid slime, and secondary ammoniation reactor |
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